CN107068996B - A kind of continuous preparation method of silicon-carbon nitrogen composite material - Google Patents
A kind of continuous preparation method of silicon-carbon nitrogen composite material Download PDFInfo
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- CN107068996B CN107068996B CN201710108854.5A CN201710108854A CN107068996B CN 107068996 B CN107068996 B CN 107068996B CN 201710108854 A CN201710108854 A CN 201710108854A CN 107068996 B CN107068996 B CN 107068996B
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Abstract
The invention discloses a kind of continuous preparation methods of silicon-carbon nitrogen composite material, are related to lithium cell cathode material synthesis field.This method comprises: metallic silicon is uniformly mixed according to a certain percentage with graphite powder；It is put into the flowing in continuous high-temperature furnace with inert protective gas after uniformly mixed metallic silicon and graphite powder are placed in graphite crucible, completes silicon and is deposited on graphite, form Si-C composite material；The Si-C composite material of formation is heated again, while carbon source and nitrogen source is added, secondary deposition is completed, obtains silicon-carbon nitrogen composite material.The present invention prepares the method for Si-C composite material by reasonable utilization waste heat save the cost, shortens process flow, so that the preparation time of silicon-carbon nitrogen composite material shortens, saves resource and cost.
Description
Technical field
The present invention relates to lithium cell cathode materials to synthesize field, more particularly relates to a kind of the continuous of silicon-carbon nitrogen composite material
Preparation method.
Background technique
Carbon material is the most widely used material of current negative electrode of lithium ion battery, its not only technique for applying technology maturation is held
Amount is higher, but also has excellent cycle performance, higher coulombic efficiency and stable discharge voltage plateau, compatible with solvent
Property it is good, high and stable operating voltage, preferable high temperature performance and security performance can be provided for lithium battery.The theory of silicon materials
Specific capacity is very high, and energy density can be improved up to 200% or more after silicon-carbon is compound, has both been able to satisfy the capacity of portable high power power supply
It is required that being also able to satisfy the high power needs that hybrid-electric car proposes lithium ion battery, and carbon material can also alleviate silicon and exist
The phenomenon that violent volume change bring inner tensions cause electrode pad material dusting to be collapsed in cyclic process.Silicon, carbon pass through
After special process composite molding, the absolute volume in charge and discharge process is varied less, and has good cycle performance and higher
Efficiency for charge-discharge, not only better performances but also relatively stable.
Silicon-carbon nitrogen composite material is very widely used at present, but its preparation time is long, and energy consumption is big, can waste many times
And resource.
Summary of the invention
The present invention provides a kind of continuous preparation method of silicon-carbon nitrogen composite material, solves to make in traditional silicon-carbon nitrogen composite material
The standby time is long, and consume energy big problem.
Specifically, in the present invention silicon-carbon nitrogen composite material continuous preparation method, comprising the following steps:
Step 1: silicon source and graphite powder being fitted into graphite crucible after evenly mixing, the molar ratio of the silicon source and graphite powder
For 0.1-5:100；
Step 2: graphite crucible being placed on to the high-temperature region of continuous high-temperature furnace, inertia protection gas is filled with into continuous high-temperature furnace
Body, and in-furnace temperature is heated, so that the mixture in graphite crucible is kept the temperature 30-120min at 2300-2500 DEG C, later by graphite
Crucible is mobile from high-temperature region to cooling area, while the flow direction for adjusting inert protective gas in furnace is flowed from high-temperature region to cooling area
It is dynamic, using inert protective gas as carrier, the silicon steam restored by carbon escaped in graphite crucible is driven to flow into from high-temperature region
Cooling area, into after cooling area, silicon steam is changed into liquid, be deposited in the form of nano-silicon or silicon nanowire graphite gaps or
Graphite surface forms Si-C composite material；
Step 3: the temperature of cooling area being down to 650-700 DEG C, then carbon source and nitrogen is added in the titration mouth of continuous high-temperature furnace
Source is added after carbon source and nitrogen source cooling area heating being heated to 750-950 DEG C, 5-30min kept the temperature, after decomposing carbon source and nitrogen source
On the quick Si-C composite material for spreading and being deposited in crucible, cooling is come out of the stove after the completion of deposition, obtains silicon-carbon nitrogen composite material.
Preferably, the silicon source selects metallic silicon, silicon monoxide or silica, and the purity of the graphite powder is 3-5N,
The granularity of the graphite powder is 325-800 mesh.
Preferably, the purity of the metallic silicon is 4-5N, and the partial size of the metallic silicon is 2-10 μm.
Preferably, inert protective gas selects argon gas.
Preferably, in step 3, the carbon source selects kerosene or methanol, and the nitrogen source selects ammonium hydroxide.
The invention has the benefit that
The continuous preparation method of silicon-carbon nitrogen composite material is shortened by reasonable utilization waste heat save the cost in the present invention
Process flow saves resource and cost so that the preparation time of silicon-carbon nitrogen composite material shortens.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
The continuous preparation method for the silicon-carbon nitrogen composite material that the embodiment of the present invention 1 provides, comprising the following steps:
Step 1: being 4N by purity, the metallic silicon and purity that partial size is 2 μm are 3N, and granularity is that the graphite powder of 325 mesh is uniform
It is fitted into graphite crucible after mixing, the molar ratio of the metallic silicon and graphite powder is 0.1:100；
Step 2: graphite crucible being placed on to the high-temperature region of continuous high-temperature furnace, nitrogen is filled with into continuous high-temperature furnace, and add
Hot in-furnace temperature makes the mixture in graphite crucible keep the temperature 30min at 2300 DEG C, later by graphite crucible from high-temperature region to drop
Warm area is mobile, while the flow direction for adjusting nitrogen in furnace is flowed from high-temperature region to cooling area, using nitrogen as carrier, drives graphite
The silicon steam escaped in crucible flows into cooling area from high-temperature region, and into after cooling area, silicon steam is changed into liquid, with nanometer
The form of silicon or silicon nanowire is deposited on graphite gaps or graphite surface, forms Si-C composite material；
Step 3: the temperature of cooling area being down to 650 DEG C, then kerosene and ammonium hydroxide is added in the titration mouth of continuous high-temperature furnace, is added
Enter and cooling area heating be heated to 850 DEG C after kerosene and ammonium hydroxide, keeps the temperature 15min, make kerosene fast decoupled as the temperature rises,
The gas fast decoupled of regional area, so that the pressure rise of regional area, carbon source and nitrogen source after decomposing kerosene and ammonium hydroxide
Gas quickly spreads and on the Si-C composite material that is deposited in crucible, and cooling is come out of the stove after the completion of deposition, and it is compound to obtain silicon-carbon nitrogen
Material.
Embodiment 2
The continuous preparation method for the silicon-carbon nitrogen composite material that the embodiment of the present invention 2 provides, comprising the following steps:
Step 1: by purity be silicon monoxide that 5N partial size is 5 μm and purity is 5N, and granularity is that the graphite powder of 800 mesh is uniform
It is fitted into graphite crucible after mixing, the molar ratio of the metallic silicon and graphite powder is 2:100；
Step 2: graphite crucible being placed on to the high-temperature region of continuous high-temperature furnace, argon gas is filled with into continuous high-temperature furnace, and add
Hot in-furnace temperature makes the mixture in graphite crucible keep the temperature 80min at 2400 DEG C, later by graphite crucible from high-temperature region to
Cooling area is mobile, while the flow direction for adjusting argon gas in furnace is flowed from high-temperature region to cooling area, using argon gas as carrier, drives stone
What is escaped in black crucible flows into cooling area from high-temperature region by the silicon steam formed after carbon reduction silicon monoxide, into cooling area
Afterwards, silicon steam is changed into liquid, and graphite gaps or graphite surface are deposited in the form of nano-silicon or silicon nanowire, forms silicon-carbon
Composite material；
Step 3: the temperature of cooling area being down to 680 DEG C, then methanol and ammonium hydroxide is added in the titration mouth of continuous high-temperature furnace, is added
Enter and cooling area heating is heated to 950 DEG C after methanol and ammonium hydroxide, keeps the temperature 5min, make methanol and ammonium hydroxide quick as the temperature rises
It decomposes, the gas fast decoupled of regional area, so that the pressure rise of regional area, carbon source and nitrogen source gas after making Methanol Decomposition
Body quickly spreads and on the Si-C composite material that is deposited in crucible, and cooling is come out of the stove after the completion of deposition, obtains silicon-carbon nitrogen composite wood
Material.
Embodiment 3
The continuous preparation method for the silicon-carbon nitrogen composite material that the embodiment of the present invention 3 provides, comprising the following steps:
Step 1: by purity be silica that 4N partial size is 10 μm and purity is 4N, and granularity is that the graphite powder of 600 mesh is equal
It is fitted into graphite crucible after even mixing, the molar ratio of the metallic silicon and graphite powder is 5:100；
Step 2: graphite crucible being placed on to the high-temperature region of continuous high-temperature furnace, argon gas is filled with into continuous high-temperature furnace, and add
Hot in-furnace temperature makes the mixture in graphite crucible keep the temperature 120min at 2500 DEG C, later by graphite crucible from high-temperature region to
Cooling area is mobile, while the flow direction for adjusting argon gas in furnace is flowed from high-temperature region to cooling area, using argon gas as carrier, drives stone
What is escaped in black crucible flows into cooling area from high-temperature region by the silicon steam formed after carbon reduction silica, into cooling area
Afterwards, silicon steam is changed into liquid, and graphite gaps or graphite surface are deposited in the form of nano-silicon or silicon nanowire, forms silicon-carbon
Composite material；
Step 3: the temperature of cooling area being down to 700 DEG C, then methanol and ammonium hydroxide is added in the titration mouth of continuous high-temperature furnace, is added
Enter and cooling area heating is heated to 750 DEG C after methanol and ammonium hydroxide, keeps the temperature 30min, make methanol and ammonium hydroxide fast as the temperature rises
Speed is decomposed, the gas fast decoupled of regional area, so that the pressure rise of regional area, carbon source and nitrogen source after decomposing ammonium hydroxide
Gas quickly spreads and on the Si-C composite material that is deposited in crucible, and cooling is come out of the stove after the completion of deposition, and it is compound to obtain silicon-carbon nitrogen
Material.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (4)
1. a kind of continuous preparation method of silicon-carbon nitrogen composite material, which comprises the following steps:
Step 1: silicon source and graphite powder being fitted into graphite crucible after evenly mixing, the molar ratio of the silicon source and graphite powder is
0.1-5:100；
Step 2: graphite crucible is placed on to the high-temperature region of continuous high-temperature furnace, inert protective gas is filled with into continuous high-temperature furnace,
And in-furnace temperature is heated, so that the mixture in graphite crucible is kept the temperature 30-120min at 2300-2500 DEG C, later by graphite earthenware
Crucible is mobile from high-temperature region to cooling area, while the flow direction for adjusting inert protective gas in furnace is flowed from high-temperature region to cooling area
It is dynamic, using inert protective gas as carrier, the silicon steam restored by carbon escaped in graphite crucible is driven to flow into from high-temperature region
Cooling area, into after cooling area, silicon steam is changed into liquid, be deposited in the form of nano-silicon or silicon nanowire graphite gaps or
Graphite surface forms Si-C composite material；
Step 3: the temperature of cooling area being down to 650-700 DEG C, then carbon source and nitrogen source is added in the titration mouth of continuous high-temperature furnace, is added
Enter and cooling area heating is heated to 750-950 DEG C after carbon source and nitrogen source, keep the temperature 5-30min, after decomposing carbon source and nitrogen source quickly
It spreads and on the Si-C composite material that is deposited in crucible, cooling is come out of the stove after the completion of deposition, obtains silicon-carbon nitrogen composite material；
The carbon source selects kerosene or methanol, and the nitrogen source selects ammonium hydroxide.
2. the continuous preparation method of silicon-carbon nitrogen composite material according to claim 1, which is characterized in that the silicon source is selected
Metallic silicon, silicon monoxide or silica, the purity of the graphite powder are 3-5N, and the granularity of the graphite powder is 325-800 mesh.
3. the continuous preparation method of silicon-carbon nitrogen composite material according to claim 2, which is characterized in that the metallic silicon
Purity is 4-5N, and the partial size of the metallic silicon is 2-10 μm.
4. the continuous preparation method of silicon-carbon nitrogen composite material according to claim 1, which is characterized in that in step 2, inertia
Protective gas selects argon gas.
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| CN108615866A (en) * | 2018-05-03 | 2018-10-02 | 无锡尼摩新能源科技有限公司 | A kind of agraphitic carbon lithium cell cathode material containing nano-silicon |
| CN109860567A (en) * | 2019-02-26 | 2019-06-07 | 成都爱敏特新能源技术有限公司 | A kind of Copper substrate graphene/silicon/carbon nitrogen combination electrode and preparation method thereof |
| CN110048092B (en) * | 2019-03-01 | 2022-05-24 | 四川翔丰华新能源材料有限公司 | Lithium battery silicon-carbon composite material and preparation method thereof |
| KR102133961B1 (en) * | 2019-04-05 | 2020-07-14 | (주)에이치피케이 | Manufacturing method of composite anode material and composite anode material for lithium secondary battery |
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